WO2008054759A2 - Composite laminaire contenant du tissu et son procédé de fabrication - Google Patents

Composite laminaire contenant du tissu et son procédé de fabrication Download PDF

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Publication number
WO2008054759A2
WO2008054759A2 PCT/US2007/022960 US2007022960W WO2008054759A2 WO 2008054759 A2 WO2008054759 A2 WO 2008054759A2 US 2007022960 W US2007022960 W US 2007022960W WO 2008054759 A2 WO2008054759 A2 WO 2008054759A2
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WO
WIPO (PCT)
Prior art keywords
fibers
composite
fiber
substrate
substrates
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Application number
PCT/US2007/022960
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English (en)
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WO2008054759A3 (fr
Inventor
Yong K. Kim
Armand F. Lewis
John M. Rice
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U Mass Dartmouth - Central
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Publication of WO2008054759A2 publication Critical patent/WO2008054759A2/fr
Publication of WO2008054759A3 publication Critical patent/WO2008054759A3/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
    • B29C70/24—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in at least three directions forming a three dimensional structure
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/024—Woven fabric
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C08J5/248—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using pre-treated fibres
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    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
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    • B32B2262/14—Mixture of at least two fibres made of different materials
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/202—Conductive
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/23907—Pile or nap type surface or component
    • Y10T428/23914—Interlaminar
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24174—Structurally defined web or sheet [e.g., overall dimension, etc.] including sheet or component perpendicular to plane of web or sheet

Definitions

  • the present disclosure relates to fabric based laminar composites showing high interlaminar strength, in particular to z-directional fiber reinforced composites.
  • OPEC Organic Polymer Engineering Composite
  • z-directional reinforcement remains highly unpredictable due to the large number of variables (e.g., fiber type, flock fiber density (the number of perpendicularly oriented flock fibers per unit area of interface between the substrates), fiber denier (mass in grams per 9000 m), fiber length, binder resin type, bonding strength between fiber and binder resin, etc.) present in such a composite.
  • fiber type the number of perpendicularly oriented flock fibers per unit area of interface between the substrates
  • fiber denier masses in grams per 9000 m
  • fiber length e.g., fiber length, binder resin type, bonding strength between fiber and binder resin, etc.
  • each composite includes adjacent substrates having a reinforcement zone disposed therebetween.
  • Each reinforcement zone includes a binder resin and a plurality of z-directional fibers extending between the substrates.
  • variables such as the type of fibers, the flock fiber density, the dimensions and/or configuration (e.g., straight, branched, etc.) of the fibers, the orientation of the fibers in the reinforcement zone, the type of binder incorporated into the reinforcement zone, etc. can be selected, modified, and/or optimized in order to provide a desired performance or characteristic of the composite such as toughness, interlaminar strength, electrical and/or thermal conductivity, or any other desired property.
  • the composite includes a plurality of substrates and a reinforcement zone disposed between adjacent substrates of the plurality of substrates.
  • the reinforcement zone can include a binder resin (e.g., an epoxy resin, an unsaturated polyester resin, a vinyl ester resin, etc.) and a plurality of fibers wherein a majority of the fibers can be oriented substantially perpendicular to the substrates such that the substantially perpendicularly oriented fibers can span adjacent substrate layers and can be embedded in the adjacent substrate layers.
  • the fibers can be dispersed in the reinforcement zone at a desired flock fiber density. Fibers disposed in the reinforcement zone can be disposed therein using an electrostatic fiber coating process called flocking.
  • textile flocking can involve a process of accelerating short fibers in an electrostatic field such that they are made to impinge on a substrate surface that is coated with an uncured (liquid) or partially cured (B-staged) adhesive layer.
  • the electric field causes these short fibers to adhere in substantially perpendicular orientation to the surface.
  • these oriented fibers are hereby fixed in place on the surface.
  • the fibers disposed in the reinforcement zone by any such flocking procedure can be oriented in various ways. For example, as indicated above, a majority of the fibers can be substantially perpendicular relative to the adjacent substrates.
  • the reinforcement zone can further include a plurality of fibers oriented at an angle to the substrates.
  • the fibers can be bent or crimped, include any amount of branching, etc.).
  • Various embodiments of the presently disclosed composite can include various types of fibers (e.g., polymer-based fibers, glass fibers, carbon fibers, natural fibers, and metal fibers) and/or fibers of various dimensions.
  • the parameters are dependent upon one another (e.g., a certain fiber type or type of binder resin will require a certain flock fiber density to provide a composite exhibiting a desired property) and can be optimized in light of the desired properties of the final composite.
  • the composite can include fibers having an average denier of about 1.5 to about 25.
  • the composite can include fibers having an average length in the range of about 0.5mm to about 5mm and/or fibers having a diameter in the range of about 7 micrometers to about 50 micrometers.
  • Another variable which can be optimized to provide a composite having the desired properties is fiber flock density.
  • the composite can include fibers being dispersed within the reinforcement zone at a flock density of about 50 fibers/mm 2 to about 600 fibers/mm 2 .
  • the fibers can include a surface treatment capable of providing or enhancing some property of the fibers.
  • the surface treatment can include a surface electrical conductivity modifying agent, an adhesion promoting agent, etc.
  • a composite which includes at least a first and second substrate layer wherein at least one of the substrates is a pre-preg having a binder resin incorporated therein. Additionally, the composite can include a plurality of fibers disposed within the binder resin of the pre-preg. Similar to above, a majority of the fibers can be oriented substantially perpendicular to the substrates such that the substantially perpendicularly oriented fibers can span the first and second substrate layers and can embed in the first and second substrate layers.
  • the binder resin can be an epoxy such as a b-staged epoxy.
  • the method includes applying a binder resin to at least one side of a substrate and delivering a plurality of fibers to the substrate by a flocking procedure capable of orienting the fibers substantially perpendicular to the substrate and at a desired flock fiber density (e.g., about 50 fibers/mm 2 to about 600 fibers/mm 2 ) such that the fibers are embedded in the substrate and extend through the binder matrix.
  • a flocking procedure can be utilized by the current procedure.
  • the flocking procedure can include electrostatic flocking, applying a magnetic field to fibers including magnetic nanoparticles, etc.
  • the method can also include fabrication of a multi-layered composite by a lay-up procedure. In other embodiments, pre-pregs can be utilized in multi-layered composite fabrication.
  • FIG. 1 schematically illustrates an exemplary embodiment of a single layer z- directional fiber based reinforced composite
  • FIG. 2 schematically illustrates an exemplary embodiment of a multi-layered z- directional fiber based reinforced composite
  • FIG. 3 schematically illustrates another exemplary embodiment of a z-directional fiber based reinforced composite
  • FIG. 4 is a graph showing pull-out force versus fiber density for various fiber types
  • FIG. 5 is a graph showing pull-out force versus displacement for various fiber types
  • FIG. 6 is a graph showing pull-out force versus flock density for various fiber types
  • FIG. 7A shows a crack tip resulting from a Double Cantilever Beam (“DCB”) test
  • FIG. 7B is a magnified view of fiber bridging near the crack tip as shown in FIG.
  • FIG. 8 is a graph showing model fracture toughness versus delamination length for various fiber types
  • FIG. 9 shows an overview of finite element modeling for a composite
  • FIG. 10 is a graph comparing finite element modeled data and actual pull-out force versus displacement data
  • FIG. 11 A shows a DCB fracture model
  • FIG. 1 IB is a graph comparing finite element modeled data and actual model- fracture toughness versus delamination length data
  • FIG. 12 is a graph showing maximum pull-out force versus fiber density for a high strength carbon fiber.
  • the present disclosure provides fiber based z-directional reinforced composites specifically configured and optimized to exhibit any number of desired properties and/or characteristics. More specifically, composites are provided having single or multiple layers in which each layer can include a reinforcement zone positioned between adjacent substrates.
  • the reinforcement zone can include a plurality of z-directional fibers dispersed within a binder resin
  • at least some of the fibers are oriented in a direction substantially perpendicular to the substrates
  • the strength, performance, and properties of the composite can be optimized by selection of fiber/binder/substrate combinations and/or optimization of numerous variables
  • Such variables can include, for example, flock fiber density, fiber surface resistivity, ratio of fiber denier to fiber length, aspect ratio of the fibers, and bonding strength of fiber to the binder resin
  • the fibers can be treated with various types of surface treatments in order to achieve the desired performance
  • FIG 1 illustrates an exemplary embodiment of a single layered z-directional fiber based composite 10 having a reinforcement zone 16 positioned between a first substrate 12 and a second substrate 14
  • the reinforcement zone 16 can include a plurality of fibers 20 dispersed within a binder resin 18 made from a material such as epoxy
  • at least some of the fibers 20 can be oriented substantially perpendicular to the substrates 12, 14
  • about 80% of the fibers 20 are substantially perpendicular to the substrates 14, 12
  • about 50%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or 100% of the fibers 20 can be oriented substantially perpendicular to the substrates 12, 14
  • any or all of the fibers 20 can be substantially straight, have some degree of a curvature, and/or have a crimp
  • the fibers 20 can be embedded in each substrate 12, 14 by any type of process capable of providing the desired result
  • the fibers 20 can be embedded in each substrate 12, 14 by any type of process capable of providing the
  • the fibers 20 may be polymer-based fibers, glass fibers, carbon fibers, natural fibers, metal fibers, or any combination thereof.
  • Exemplary polymer-based fibers include those made from polyester (e g, polyethylene terephthalate (“PET”) fiber), polybutylene terephthalate (“PBT”)), nylons (nylon 6, 6-6, 3, 6-10), rayons, cellulosic fibers, polyvinylacetate fibers, polyimide and polyaramides (e.g., Nomex® or Kevlar®).
  • Exemplary natural fibers include cotton, jute and other bast fibers.
  • Examples of metal fibers include stainless steel fibers, titanium fibers, nickel fibers, copper fibers, brass . fibers, bronze fibers, or any such alloys. In one embodiment, the fibers are nanostructures.
  • such nanostructures can include a magnetic material (e.g., nickel, cobalt-nickel, etc.) capable of responding to a magnetic field.
  • a magnetic material e.g., nickel, cobalt-nickel, etc.
  • the fibers can have a wide range of dimensions. However, as indicated above, careful selection and optimization of such dimensions in relation to various other variables (e.g., type of fiber, type of binder resin, type of substrate, etc.) can provide a desired range of properties for a resulting composite.
  • the fibers can have a length to denier ratio (measured as length to diameter ratio for certain fibers) in the range of about 1 to about 10.
  • Exemplary fibers have an average denier in the range of about 0.2 to about 25 and an average length in the range of about 0.5 mm to about 5mm.
  • the fibers can be subjected to a surface treatment thereby enhancing the performance of the composite.
  • any surface treatment capable of modifying the characteristics of the fiber and/or composite e.g., interaction of the fibers with the binder resin
  • the surface treatment can include a surface electrical conductivity modifying agent and/or an adhesion promoting/degrading agent.
  • the surface electrical conductivity modifying agents can be used as fiber surface activity agents that enhance the flockability of the fibers.
  • electrical activity agents include quaternary ammonium and poly-tannic acid compounds, metallic ionic compounds, and carbon black. These surface agents serve as humectants and ionic conduction compounds, which absorb moisture for changing the electrical conductivity of the flock fiber's surface thereby effecting the flock "activity" of the fiber. These humectant surface chemicals may assist in the electro-coating or flock processing of these z-direction reinforcement fibers.
  • the surface treatment agent can also include an adhesion promoting agent configured to increase the bonding strength between the fibers and binder resin (e.g., epoxy resin).
  • binder resin e.g., epoxy resin
  • the adhesion promoting agent can include strong oxidizing acids for carbon fibers, and coupling agents for specific resins such as epoxy functional silane compounds.
  • Adhesion degrading agents can be used when it is desirable to reduce the fiber/binder matrix adhesion strengths.
  • fluorocarbon based surface energy reducing agents can be used.
  • the substrates 12, 14 can be formed from a wide range of materials.
  • the substrate can be formed from a unidirectional filament sheet, a woven fabric, glass fiber, carbon and/or any other type of advanced fiber.
  • the substrate may be formed from a pre-impregnated composite fiber ("pre-pregs").
  • Pre-pregs typically take the form of woven or uni-directional fibers that are bound in a matrix material (e.g., a b-staged resin matrix material).
  • Pre-pregs are typically stored under refrigerated, frozen conditions at about -2O 0 C. Storing these pre- pregs under cold conditions extends their storage-to-processing use time.
  • the pre-pregs When ready to use, the pre-pregs are removed from the freezer, brought to room temperature (with care being taken so that moisture does not condense on the pre-pregs's surface — to avoid such condensation, the pre-pregs should be wrapped in an aluminum foil (or the like) while it is warming to room temperature), manipulated into the desired laminar structure, and finally cured in a forming press or vacuum bag under heat.
  • the curing agents in these matrix resins are commonly activated by heat.
  • An exemplary pre-preg is Cycom 934, available from Cytec Industries (Greenville, Texas).
  • An advantage of using a pre-preg substrate is that fibers may be flocked directly onto the pre-preg without the addition of a binder resin.
  • the pre-preg includes a "b-staged" epoxy capable of engaging the fibers.
  • the pre- preg is heated to render the resin matrix of the pre-preg more fluid (less viscous) so the flock fibers can better penetrate and embed themselves in the pre-preg.
  • both sides of the pre-preg may be flocked and placed between adjacent substrates.
  • the adjacent substrates may include, for example, a polyethylene/polyethyleneteterfluoride ("PTFE”) release film, an adhesional pre-preg, a resin impregnated fabric, or a sheet molding compound
  • the binder resin 18 of the composite 10 can include any of a number of materials which exhibit adhesive properties.
  • the binder resin 18 can be an epoxy resin, an unsaturated polyester resin, and/or a vinyl ester resin.
  • the binder resin is an epoxy resin.
  • a useful epoxy resin can include about
  • Epon 826 Shell Chemical Co.
  • Epicure 3223 curing agent Shell Chemical Co.
  • the binder resin is Cycom 997 resin (commercially available from Cytech Industries).
  • Other useful epoxy resins include amine cured (liquid) epoxy resins, Dicy cured epoxy resins, and anhydride cured (liquid) epoxy resins.
  • FIG. 2 illustrates an exemplary embodiment of a multi-layered composite 10' having substrates 12, 14, 30, 32, each separated by a reinforcement zone 16, 34, 36.
  • first and second substrates 12, 14 can be separated by a first reinforcement zone 16, second and third substrates 14, 30 can be separated by a second reinforcement zone 34, and third and fourth substrates 30, 32 can be separated by a third reinforcement zone 36.
  • Each reinforcement zone 16, 34, 36 can include a plurality of fibers 20 disposed within a binder resin matrix 18 such that the fibers 20 are oriented substantially perpendicular to their corresponding substrate layers 12, 14, 30, 32.
  • the multi-layered composite 10' is shown to include four substrate layers and three reinforcement zones, those skilled in the art will appreciate that the multi-layered composite 10' can include any desired number of layers. Additionally, such multi-layered composites can also include pre-preg(s). In some embodiments, an outer surface of the pre-preg can be coated with an epoxy coating (e.g., an epoxy coating having a thickness of about 0.001 inches to about 0.008 inches) before the pre-preg is layered onto a flock covered ply. Such fabrication procedures will be further described below.
  • an epoxy coating e.g., an epoxy coating having a thickness of about 0.001 inches to about 0.008 inches
  • multi-layered composites 10' can use a single type of binder resin or different types of binder resin. Additionally, multi-layered composites 10' may use a single type of substrate or various types of substrates formed of different materials. Likewise, various types of fibers or a single fiber-type may be used in a multi-layered composite 10'.
  • fibers can be arranged so they penetrate through both sides of a carrier substrate (i.e., pass through the carrier substrate).
  • This z-direction veil or scrim substrate can then be used as an interply layer between adjacent substrates or pre-pregs.
  • the carrier layer imparts the z-directional reinforcement in the laminar composite.
  • FIG. 3 illustrates another embodiment of a single layer composite 100 having fibers 20 that are substantially perpendicular to each substrate 12, 14, as well as other fibers that are not substantially perpendicularly oriented. That is, the reinforcement zone 16 can include fibers 50 positioned at an angle to the substrates 12, 14. Additionally, the fibers 20, 50 can optionally include fiber branches 52 that can be oriented in a variety of directions.
  • the composite 100 having a reinforcement zone with non-perpendicular and/or branched fibers, can also be used to form multi-layered composites.
  • a multi-layered composite can include reinforcement zones having fibers that are all substantially perpendicularly oriented as well as reinforcement zones with fibers that are non-perpendicular (e.g., fibers having an oblique orientation angle distributed between about 45 degrees and about 135 degrees).
  • the composite can be fabricated by initially determining a set of desired properties and further selecting and/or modifying the fibers, binder resin, and/or substrate(s) in order to provide such properties.
  • the fibers can be selected and/or modified to exhibit a surface resistivity of about 1 x 10 5 ohms to about 1 x 10 9 ohms.
  • Such fibers can also be selected and/or modified to have an aspect ratio (length/diameter) in the range of about 100 to about 1000 or higher.
  • Various other embodiments can utilize fibers of various other characteristics and/or properties in order to exhibit some desired composite performance.
  • the composite In selecting an optimal fiber/binder combination, it is desirable for the composite to have an optimal bonding strength between the fibers and the binder resin. If the bonding strength between fiber and binder is too high, then the composite will delaminate at the fabric/binder interface as fibers will be broken and pulled out during crack growth. If the bonding strength is too low then the force and corresponding energy required for the fiber pull out will be small, therefore during the pull out there will be insufficient crack growth energy reduction.
  • the flock fiber density is dependent upon fiber denier. For example, fibers of a diameter in the range of about 20 micrometers to about 50 micrometers have a optimum flock density of about 125 fibers/mm 2 to about 250 fibers/mm 2 . However, fibers having diameters in the range of about 7 micrometers to about 10 micrometers have an optimum flock fiber density of about 200 fibers per mm 2 to about 800 fibers per mm 2 . If the flock fiber density falls below the optimum density range for the particular fiber, the force and corresponding energy required to pull out the fibers will be relatively small during fiber pull-out resulting in insufficient crack growth energy reduction. However, if the fiber density is above the optimum range for the fiber, the force and corresponding energy required to pull out the fibers is nearly constant no matter how large the density is above the range, therefore fiber inclusion is wasted above this flock density range.
  • the composites can be optimized to exhibit a desired electrical and/or thermal conductivity.
  • the electrical conductivity of a composite can be optimized by varying the flock fiber density and length of the fiber.
  • the thermal conductivity and the coefficient of thermal expansion of the composite can be optimized. For example, positioning z- directional copper fibers in a carbon or glass fabric/epoxy composite can increase the thermal conductivity and also increase the thickness of the composite as the temperature increases. Alternatively, positioning carbon fibers in a glass fabric composite can decrease the thickness of the composite as the temperature increases.
  • a method for fabricating a z-directional fiber based reinforced composite is also provided herein.
  • the method can include applying a binder matrix to at least one side of a substrate followed by delivery (e.g., flocking) of fibers to the substrate.
  • delivery e.g., flocking
  • any of a number of delivery/flocking procedures can be utilized to deliver the fibers to the substrate.
  • the fibers can be delivered by a flocking procedure, such as electrostatic flocking, which serves to embed fibers in the first substrate.
  • electrostatic flocking utilizes an electrostatic field to orient and propel the fibers so that they can be embedded into the substrate in a desired orientation (e.g., substantially perpendicular). While virtually any such apparatus can be utilized, in an exemplary embodiment the electrostatic flocking apparatus is a Model HEKl 00 Flocking Unit Magg
  • the flocking procedure can apply a magnetic field to a plurality of magnetic nanoparticle fibers.
  • the above-identified steps of applying the binder and flocking may be repeated several times to produce additional layers. Each time an additional layer is produced it is stacked upon previously formed layers until a composite with the desired number of layers is formed.
  • pressure can be applied thereto until the desired thickness of the composite is attained.
  • the pressure can additionally serve to embed the fibers in the second, adjacent substrate.
  • the desired pressure can be applied to the composite by a wide range of mechanisms. For example, pressure in the range of about 1 atmosphere to about 9 atmospheres can be applied to the composite by a platen press. In such an embodiment, the composite can be allowed to cure while still under pressure in the press. Curing, for example, can be performed overnight at room temperature. Following curing, the composite can undergo a post-cure treatment at about 8O 0 C for about 2 hours. In another embodiment, pressure can be applied to the composite using a vacuum bag.
  • the composite can be allowed to cure overnight at room temperature using a vacuum bag, followed by the post-cure treatment in an oven at about 8O 0 C for about 2 hours.
  • the following experiment compared a non-flocked composite (no z-directional reinforcing fibers) versus composites having nylon (high density and low density) and composites having polyester (treated and untreated) z-directional reinforcing fibers.
  • the reinforced composites utilized an epoxy having 100 parts Epon 826 (Shell Chemical Co., Houston, TX) mixed with 26 parts of Epicure 3223 curing agent (Shell Chemical Co.), in combination with a fiberglass substrate.
  • Mode I and Mode II fracture toughness, respectively, was observed as compared to conventional non-flocked (no fibers) glass fabric/epoxy composites; • the in-plane properties, tensile, shear, and impact strength, were found to increase in response to the selection of various desired properties (i.e., selection of about 150-250 fibers/mm 2 flock density of nylon fiber and selection of about 20-85 fibers/mm 2 flock density of treated PET fiber); there was little degradation of these in-plane properties;
  • FIG. 4 shows the results of an experiment wherein Nylon fiber's pull-out force is nearly constant at approximately 120 N for fiber densities greater than about 150 fibers/mm 2 .
  • the optimum fiber density for this 3 denier nylon fiber is about 150 to about 200 fibers/mm 2 .
  • Fiber pull-out tests were performed on flocked plates.
  • the fibers were flocked to a plate with a thin epoxy resin layer (an amine cured epoxy matrix resin (Fiberglast
  • Epoxy resin 2000/ Cure 2060 Epoxy resin 2000/ Cure 2060
  • the substrate was a 0.025 inch thick aluminum metal sheet of about 37 mm thickness, and the free ends were bonded to small disks using a hot melt adhesive. After the adhesive set, the specimens were pulled by a test apparatus. From these tests, typical force versus displacement curves were obtained for carbon, nylon, polyester ('PET”), and treated PET fiber samples at different densities, as shown in FIG. 5. The dissipation energy during fiber pull-out is proportional to the area under the curve.
  • Treated PET fibers were produced as follows: Fiber material: 3 denier PET fibers.
  • Rainoff® chemical and water is calculated by multiplying the weight of the pouch by 30, which is the liquor to material ratio.
  • the amount of Rainoff® chemical is about 0.5% of the weight of the flock fiber pouch.
  • a hair dryer is used to dry the pouch from the outside; flock fibers are transferred from the cotton cloth pouch to the polyester cloth pouch; the pouch is then dried in oven for 3 days at about 8O 0 C.
  • FIG. 5 shows that untreated nylon and polyester (PET) flock fibers behave quite similarly in their fiber pull-out force/strength tests. Pull out force is indicative of the degree of adhesion between the flock fiber and the epoxy resin polymer into which the fiber is imbedded (i.e., bonded). Treated PET flock fibers show the highest fiber pull- out force/strength among all fibers tested.
  • PET nylon and polyester
  • Double Cantilever Beam (“DCB”) tests were used in Mode I fracture toughness tests.
  • FIG. 7A shows a crack tip and FIG. 7B shows fiber bridging near the crack tip.
  • Fracture toughness versus delamination length curves were plotted from the data of the DCB tests for various fibers. These test results are shown in FIG. 8 and the data is also transposed into Table 2 below to more clearly represent the merits of z-direction flocked laminar composites in increasing the interlaminar shear strength of laminar composites.
  • Nylon and Treated PET fiber flocked glass fabric laminar composites were found to have the highest Fracture Toughness (interlaminar shear strength) among the composites tested.
  • the un-flocked laminates and the controls have a fracture toughness that is only half the fracture toughness of these z-reinforced composites.
  • FIG. 9 demonstrates how pull-out test was modeled using the finite element method.
  • the fibers were modeled using spring-slider elements.
  • a "breakaway" feature is available to allow the element stiffness to drop to about zero once a limiting force has been reached, which simulates the fiber bundles being pulled out.
  • the FE model fits the experimental data for the pull-out test very well, as shown in FIG. 10 by a typical comparison of the FE model and the pull-out curve for a high density nylon sample.
  • the energy release rate which is the change of strain energy required to open new crack areas, can be calculated from equation (1) below:
  • a finite element analysis was performed to model the Mode I failure mechanism and fracture toughness in a Double Cantilever Beam (DCB) test by using a 3-D symmetric finite element model with composite and spring-slider elements, as shown in FIG. 11 A.
  • the finite element model showed that the delamination resistance increases from the energy consumption by pull-out and/or breaks of the z-directional reinforcement fibers.
  • the model and result for z-reinforcement of about 1.3 mm-3 denier nylon fibers at about 200 fibers per mm 2 are shown in FIG. 11 B.
  • the result shows that the Mode I toughness of the z-reinforced laminar laminar composites can be explained by the fiber pulling and bridging mechanisms.
  • the multi-fiber pull-out test reflects the effect of the interaction of adjacent fibers and their surrounding epoxy resin, compared with the single fiber pull-out test, the multi-finer pull test is a better way to model local flock fiber behavior during fiber bridging in a DCB test;
  • the multi-finer pull out test shows that the maximum pull out force is a quadratic function of the fiber density. The maximum force reaches nearly a constant at some specified fiber density depending of the type of the fiber. This means that to obtain the highest fracture toughness of the flock fiber reinforced composite, the optimum density should be applied;
  • Studies on the multi-fiber, pull-out test shows that fibers with different embedded angles have a different debonding force.
  • the Poisson's ratios of these composites are around about 0.3; (7) There is no significant difference in the in-plane shear strength between the 3 denier nylon flocked composite and the non-flocked composites; and (8)
  • the DCB test is modeled using a 2D finite element model. A softening linear bridging law is used to simulate the behavior of the flocked fibers. The computational results prove this model is suitable to simulate the mode I fracture toughness in flock fiber reinforced composites.
  • the FE model also confirms that the fracture toughness is a function of the fiber pull-out stiffness and fiber bridging length.
  • the z-directional carbon fiber was an un-sized type T-300 carbon fiber with a diameter of 7 micrometers ( ⁇ m) and a fiber material density of 1.8 g/cm 3 .
  • the pre- preg was a carbon fabric/epoxy pre-preg material (CYCOM 934).
  • a typical composite was fabricated by laying up an 8 ply quasi-isotropic laminates composed of a 0/90/+45/-45/-45/+45/90/0 layering of the pre-preg plies with flocked fiber in between each layer.
  • Four composite panels were fabricated and their flock density ranges are shown in Table 4.
  • 2.54 x 2.54 cm specimens were cut from the composites, one for each of four configurations: (1) 0.5mm low density, (2) 0.5mm high density, (3) 1.0mm low density, and (4) 1.0mm high density.
  • the resistance of each specimen was measured using a multimeter equipped with probes. The multimeter probes were place on the top and bottom of the specimens in order to determine the resistance through the composite layers. Six measurements were taken for each specimen and an average and +/- standard deviation was calculated. The results of this experiment are shown in Table 5.

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Abstract

L'invention concerne des composites renforcés dans la direction z contenant des fibres possédant une meilleure résistance inter laminaire, résistance aux chocs, de meilleures propriétés de transmission (conduction électrique et thermique) et un meilleur coefficient de dilatation thermique. Les composites contiennent au moins deux substrats séparés par une zone de renfort contenant une pluralité de fibres incorporées dans un liant résineux. Au moins certaines - et dans un mode de réalisation, une majorité - des fibres sont orientées de manière à être sensiblement perpendiculaires aux substrats. Des composites multicouches possédant plus de deux couches de substrat peuvent également être formés. L'invention propose également des procédés de formation de composites de ce type.
PCT/US2007/022960 2006-10-31 2007-10-31 Composite laminaire contenant du tissu et son procédé de fabrication WO2008054759A2 (fr)

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WO2017208017A1 (fr) * 2016-06-02 2017-12-07 Gerard Fernando Matériau en feuille composite
CN109153222A (zh) * 2016-06-02 2019-01-04 杰勒德·费尔南多 复合片材材料
US11167524B2 (en) 2016-06-02 2021-11-09 Gerard Fernando Composite sheet material

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